CN109208028A - A kind of preparation method for decomposing the nitrogen of water performance improvement, phosphide - Google Patents
A kind of preparation method for decomposing the nitrogen of water performance improvement, phosphide Download PDFInfo
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- CN109208028A CN109208028A CN201811249369.0A CN201811249369A CN109208028A CN 109208028 A CN109208028 A CN 109208028A CN 201811249369 A CN201811249369 A CN 201811249369A CN 109208028 A CN109208028 A CN 109208028A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
一种分解水性能改善的氮、磷化物的制备方法，本发明涉及了改善现有电催化剂分解水催化活性低的问题，而提供一种分解水性能改善的氮、磷化物的制备方法。制备方法：一、将泡沫镍裁成小长方体，依次置于丙酮、盐酸及蒸馏水溶液中超声清洗，得到预处理泡沫镍；二、将一定量偏钒酸铵溶解在一定体积比的水和乙醇混合溶液中，通过缓慢滴加浓盐酸调节pH呈酸性，溶液颜色变成红色，形成钒多酸簇中间体；三、将步骤二的反应液转移到水热釜中，放入预处理泡沫镍水热处理。生成氧化钒/泡沫镍复合体；四、将氧化钒/泡沫镍复合体进行氮化或磷化处理，自然冷却，得到钒镍双金属氮、磷化物/泡沫镍复合体。
A method for preparing nitrogen and phosphide with improved water splitting performance, the invention relates to improving the problem of low catalytic activity of existing electrocatalysts for splitting water, and provides a method for preparing nitrogen and phosphide with improved water splitting performance. Preparation method: 1. Cut nickel foam into small rectangular parallelepipeds and place them in acetone, hydrochloric acid and distilled aqueous solution for ultrasonic cleaning in turn to obtain pretreated nickel foam; 2. Dissolve a certain amount of ammonium metavanadate in a certain volume ratio of water and ethanol In the mixed solution, the pH is adjusted to be acidic by slowly dropping concentrated hydrochloric acid, and the color of the solution turns red to form a vanadium polyacid cluster intermediate; 3. Transfer the reaction solution in step 2 to a hydrothermal kettle, and put it into the pretreated nickel foam Hydrothermal treatment. The vanadium oxide/foamed nickel composite is formed; 4. The vanadium oxide/foamed nickel composite is subjected to nitridation or phosphating treatment, and then naturally cooled to obtain a vanadium-nickel bimetallic nitrogen, phosphide/foamed nickel composite.
Description
Technical field
The present invention relates to a kind of preparation method of composite material, especially a kind of nitrogen, phosphide for decomposing water performance improvement
Preparation method.
Background technique
Hydrogen Energy is a kind of extremely superior secondary energy sources, has many advantages, such as high energy, green, environmental protection.Currently, electrochemical catalysis
Decompose water be it is a kind of cleaning, efficient hydrogen production process.Water electrolysis includes in the evolving hydrogen reaction (HER) of cathode and in the analysis oxygen of anode
It reacts (OER), theoretically thermodynamics decomposes the starting voltage that water at least needs 1.23V.However, it is contemplated that kinetics because
Element generates overvoltage effect, actually needs bigger starting voltage, the voltage that business electrolyzer generally uses for 1.8~
2.4V.In order to overcome this big overvoltage, it is urgent for finding the catalyst that a kind of couple of HER and OER all has preferable catalytic effect
In the eyebrows and eyelashes.However, that is reported so far reacts the bifunctional material with catalytic activity and few, table to HER and OER
The design synthesis of bright this kind of material is still a challenging job.
In the recent period, transition metal nitrogen, phosphide (MNC and MPC) are since the catalytic activity of its " eka-platinium " is in electrochemical decomposition water
Field causes extensive research boom.But the usual process of electrode production process of traditional MNC and MPC material is relatively multiple
It is miscellaneous and time-consuming, include mainly synthetic powder presoma and subsequent nitridation or phosphorating treatment, is collecting finally by adhesive load
On fluid.Whole process is not only laborious but also is difficult to make catalyst that uniform close is fixed and formed tightly with collector on the electrode
Contiguity touching.This result will lead to MNC the and MPC catalyst in water splitting processes and be detached from from collector, so as to cause catalysis
Activity is low with stability.In order to solve this problem, a large amount of research work concentrates on directly growing electro-catalysis on a current collector
Agent.However, the electrode stability due to caused by the bad contact between complicated manufacturing process and catalyst and collector
Decline seriously limits further applying for such electrode.Therefore, simple, expansible, efficient nitrogen, phosphide electro-catalysis are explored
The synthetic method of agent is commercially used for having important theoretical and practical significance realize electrochemical decomposition water.
Summary of the invention
The invention aims to improve existing elctro-catalyst to decompose the low problem of aqueous energy catalytic activity, and provide one kind
Decompose the nitrogen of water performance improvement, the preparation method of phosphide.
Transition metal nitrogen of the present invention, phosphide complex preparation method follow these steps to realize:
Nickel foam, is cut into small cuboid by step 1, is then sequentially placed into acetone, distilled water and hydrochloric acid solution and is surpassed
Sound cleaning, is washed with distilled water again later, is placed in drying in baking oven, obtains pretreated nickel foam；
A certain amount of ammonium metavanadate is dissolved in the water of certain volume ratio and the solution mixed liquor of ethyl alcohol by step 2, acute
Strong stirring.PH value of solution is adjusted in acidity by being slowly dropped into concentrated hydrochloric acid, and solution colour becomes red, is formed among vanadium polyacid cluster
Body；
Step 3, the reaction solution that step 2 is obtained are transferred in the water heating kettle with polytetrafluoroethyllining lining, then again
It is put into pretreatment nickel foam hydro-thermal process, generates vanadium oxide/froth nickel complex；
Vanadium oxide/nickel foam complex is put into tube furnace and carries out nitridation or phosphorating treatment, then with furnace by step 4
Natural cooling obtains vanadium nickel bimetal nitrogen, phosphide/froth nickel complex.
The present invention passes through a kind of simple, expansible, efficient nitrogen, phosphide electrocatalyst materials.Gained of the invention
Nitrogen, phosphide electrocatalyst materials due to good electrocatalytic decomposition it is aqueous can, vanadium nickel bimetal nitride/nickel foam is compound
Body surface reveals excellent HER catalytic activity, and starting overpotential is 0mV, in 10mA cm-2Current density under overpotential difference
For 64mV.It is noted that vanadium nickel bimetal nitride/foamed nickel catalyst agent activity is even better than business Pt/C catalysis
Agent.This shows that vanadium nickel bimetal nitride/foamed nickel catalyst agent may be used as efficient base metal and produce hydrogen catalyst, meanwhile,
Vanadium nickel bimetal phosphide/nickel foam shows excellent OER catalytic activity, onset potential 1.45V, in 100mA cm-2's
Overpotential under current density is respectively 1.63V.It should also be mentioned that vanadium nickel bimetal phosphide/foamed nickel catalyst agent
Activity be better than Ru/C catalyst.This shows that vanadium nickel bimetal phosphide/nickel foam may be used as efficiently producing VPO catalysts.
In summary the present invention also comprising following the utility model has the advantages that
1. it is environmentally friendly, inexpensive that any adhesive is not used in the present invention.
2. the present invention is by passing through collector (nickel foam, foamed iron) slow release transition metal ions (Ni, Fe in situ
Deng) strategy make in conjunction with the late transition metals component such as vanadium and Ni (Fe).Operating procedure is simple, low energy consumption, and needed for reaction
Equipment is simple, is conducive to the large scale preparation of material.
3. the present invention can be by adjusting preparation parameter (material rate), transition metal source (Ni, Co, Fe etc.), heat treatment
Condition (hydrothermal condition and calcination condition etc.) is realized to bimetallic in vanadium bimetallic nitrogen, phosphide/nickel foam, iron complex
The regulation of nitrogen, the size of phosphide, pattern, metal ratio, active sites.
Detailed description of the invention
Fig. 1 is vanadium nickel bimetal nitride/froth nickel complex transmission electron microscope figure that embodiment one obtains；
Fig. 2 is vanadium nickel bimetal nitride/froth nickel complex powder x-ray diffraction spectrogram that embodiment one obtains；
Fig. 3 is vanadium nickel bimetal phosphide/froth nickel complex transmission electron microscope figure that embodiment one obtains；
Fig. 4 is vanadium nickel bimetal phosphide/froth nickel complex powder x-ray diffraction spectrogram that embodiment one obtains；
Fig. 5 is the Hydrogen Evolution Performance of different catalysts；
Fig. 6 is the analysis oxygen performance of different catalysts；
Fig. 7 is the polarization curve of two electrode complete solution water.
Specific embodiment
Specific embodiment 1: the preparation method of present embodiment transition metal nitrogen, phosphide complex follows these steps
It realizes:
Nickel foam, is cut into small cuboid by step 1, is then sequentially placed into acetone, distilled water and hydrochloric acid solution and is surpassed
Sound cleaning, is washed with distilled water again later, is placed in drying in baking oven, obtains pretreated nickel foam；
A certain amount of ammonium metavanadate is dissolved in the water of certain volume ratio and the mixed solution of ethyl alcohol, acutely by step 2
Stirring.By being slowly dropped into concentrated hydrochloric acid for pH value of solution in acidity, solution colour becomes red, forms vanadium polyacid cluster intermediate；
Step 3, the reaction solution that step 2 obtains are transferred in the water heating kettle with polytetrafluoroethyllining lining, then put again
Enter to pre-process nickel foam hydro-thermal process.Generate vanadium oxide/froth nickel complex；
Vanadium oxide/nickel foam complex is put into tube furnace and carries out nitridation or phosphorating treatment, then with furnace by step 4
Natural cooling obtains vanadium nickel bimetal nitrogen, phosphide/froth nickel complex.
Transition metal nitrogen, phosphide complex obtained by present embodiment, transition metal nitrogen, phosphide are in foamed nickel current collector
Homoepitaxial, transition metal nitrogen, phosphide such as contact at the advantages with collector, show excellent complete solution water catalytic activity and steady
It is qualitative.
Specific embodiment 2: the present embodiment is different from the first embodiment in that nickel foam is cut into ruler by step 1
The very little small cuboid for 4cm × 3cm.Other steps and parameter are same as the specific embodiment one.
Specific embodiment 3: step 2 water and second unlike one of present embodiment and specific embodiment one to two
The mixed liquor volume ratio of alcohol is 1:(1~20).Other steps and parameter are identical as one of specific embodiment one to two.
Specific embodiment 4: step 2 presses inclined vanadium unlike one of present embodiment and specific embodiment one to three
The mass ratio of sour ammonium and solvent is 1:(50~200) by the mixed solution of ammonium metavanadate to water and ethyl alcohol, obtain ammonium metavanadate
Solution.Other steps and parameter are identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four described in step 2
By be slowly dropped into concentrated hydrochloric acid by solution ph be 1~5.Other steps and one of parameter and specific embodiment one to three phase
Together.
Specific embodiment 6: water described in step 3 unlike one of present embodiment and specific embodiment one to five
The temperature of heat treatment is 120~180 DEG C.Other steps and parameter are identical as one of specific embodiment one to five.
Specific embodiment 7: water described in step 3 unlike one of present embodiment and specific embodiment one to six
The hydro-thermal time of heat treatment is 8~24 hours.Other steps and parameter are identical as one of specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven at step 4 nitridation
The temperature of reason is 400~700 DEG C, and nitridation time is 1~4 hour.Other steps and parameter and specific embodiment one to seven it
One is identical.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight at step 4 phosphatization
The temperature of reason is 400~700 DEG C, and phosphating time is 1~4 hour.Other steps and parameter and specific embodiment one to eight it
One is identical.
Embodiment one: the present embodiment transition metal nitrogen, phosphide complex preparation method follow these steps to realize:
Nickel foam is cut into the small cuboid having a size of 4cm × 3cm by step 1, be then sequentially placed into acetone, distilled water with
And it is cleaned by ultrasonic 15min in hydrochloric acid solution, it is washed with distilled water again several times later, is placed in drying in baking oven, is pre-processed
Nickel foam；
The ammonium metavanadate of 0.2g is dissolved in the mixed solution of water and ethyl alcohol (alcohol: water volume ratio 1:9) by step 2,
By being slowly dropped into concentrated hydrochloric acid for pH value of solution in 2, solution colour becomes red, is vigorously stirred, and forms vanadium polyacid cluster intermediate；
Step 3, the reaction solution that step 2 is obtained are transferred in the water heating kettle with polytetrafluoroethyllining lining, then again
It is put into pretreatment nickel foam, hydro-thermal process temperature is 160 DEG C, and the hydro-thermal time is 10 hours, and it is compound to obtain vanadium oxide/nickel foam
Body.
Vanadium oxide/nickel foam complex is put into tube furnace and carries out nitridation or phosphorating treatment, calcination temperature by step 4
It is 600 DEG C, phosphating time is 2 hours, and then with furnace natural cooling, it is compound to obtain vanadium nickel bimetal nitrogen, phosphide/nickel foam
Body.
Fig. 1 shows vanadium nickel bimetal nitride/froth nickel complex scanning electron microscope diagram piece, can from figure
To find out, it may be clearly seen that the array structure of vanadium nickel bimetal nitride particles assembling is equably grown in nickel foam afflux
On body, particle size is about 5nm.Proof forms tungsten nitride/graphene-carbon nano tube composite material of small size, high dispersive.
Fig. 2 shows vanadium nickel bimetal nitride/froth nickel complex powder x-ray diffraction spectrogram, can be with from figure
Find out that 2 θ are 38.9 °, 42.3 °, 44.4 °, 58.5 °, 70.6 ° and 78.4 ° and belong to Ni3(110) of N (PDF#10-0280),
(002), (111), (112), (300) and (113) crystal face diffraction.VN is respectively designated as at 37.9 °, 43.9 °, 64.3 ° and 76.6 °
(PDF#65-7236) (111), (200), (220) and (311) crystal face diffraction.Strong peak at 44.7 °, 52.1 ° and 76.7 °
(111), (200) and (220) crystal face diffraction of W metal (PDF#65-2865) from foam Ni substrate, it was demonstrated that vanadium nickel is double
Metal nitride/froth nickel complex is successfully prepared.
Fig. 3 shows vanadium nickel bimetal phosphide/froth nickel complex scanning electron microscope diagram, can from figure
Vanadium nickel bimetal phosphide nanoscale twins oldered array is grown in foamed nickel current collector out, the thickness of lamella is about
10nm, and some nanoparticles are grown in lamella array surface, partial size is about that 6nm proof forms small size, high dispersive
Tungsten nitride/graphene-carbon nano tube composite material.
Fig. 4 shows vanadium nickel bimetal phosphide/froth nickel complex powder x-ray diffraction spectrogram, these diffraction maximums
It is respectively belonging to Ni2P(PDF#65-9706)、VP2(PDF#30-1426) and the feature diffraction of simple substance Ni (PDF#65-2865)
Peak, it was demonstrated that successfully prepare vanadium nickel bimetal phosphide/froth nickel complex.
Fig. 5 show be different catalysts Hydrogen Evolution Performance, under room temperature using classical in 1.0M KOH solution
Three-electrode system has rated the performance of vanadium nickel bimetal nitrogen, phosphide/froth nickel complex catalysis HER.Nickel foam is used simultaneously
It is as a comparison sample with business Pt/C.In 5mV s-1To sweep nickel foam under speed, vanadium nickel bimetal nitride/nickel foam, vanadium nickel double
The polarization curve of metal phosphide/nickel foam and Pt/C catalyst.It can be seen from the figure that the HER activity of nickel foam is poor, and
Vanadium nickel bimetal nitride/nickel foam, vanadium nickel bimetal phosphide/nickel foam show excellent HER catalytic activity, originate
Potential distinguishes 57 and 0mV, and cathode-current density is increased rapidly with the increase of overpotential, in 10 and 100mA cm-2Electricity
Overpotential under current density is respectively 147,319 and 64,218mV.It is noted that vanadium nickel bimetal nitride/nickel foam
The activity of catalyst is even better than business Pt/C catalyst.This shows that vanadium nickel bimetal nitride/nickel foam may be used as efficiently
Base metal produce hydrogen catalyst.
Fig. 6 show be different catalysts analysis oxygen performance, it is same we also in 1.0M KOH solution under room temperature
The performance of vanadium nickel bimetal nitrogen, phosphide/froth nickel complex catalysis OER is had rated using classical three-electrode system.Fig. 6
It gives in 5mV s-1Sweep nickel foam under speed, vanadium nickel bimetal nitride/nickel foam, vanadium nickel bimetal phosphide/nickel foam
With the polarization curve of Ru/C catalyst.It can be seen in the drawing that the OER activity of nickel foam is poor, and vanadium nickel bimetal nitride/
Nickel foam, vanadium nickel bimetal phosphide/nickel foam show excellent OER catalytic activity, and onset potential shows 1.45 respectively
With the starting overpotential and 100mA cm of 1.50V-2Current density under overpotential be respectively 1.63 and 177V.It is same to be worth
One is mentioned that, vanadium nickel bimetal phosphide/foamed nickel catalyst agent activity is better than Ru/C catalyst.This shows vanadium nickel bimetal
Phosphide/nickel foam may be used as efficiently producing VPO catalysts.
In order to which closer to practical application, we use vanadium nickel bimetal phosphide/nickel foam as anode and vanadium nickel respectively
Bimetallic nitride/nickel foam is as two electrolysis hydrophone part of cathode assembling.Fig. 7 show be two electrode complete solution water polarization
Curve, two electrodes to vanadium nickel bimetal phosphide/nickel foam as anode and vanadium nickel bimetal nitride/nickel foam conduct
The lower onset potential of two electrode complete solution water of cathode assembling is only 1.43V.It also, is 10mA cm in current density-2When apply
Voltage be only 1.51V, the above result shows that vanadium nickel bimetal nitrogen, phosphide/nickel foam have in complete solution water it is potential practical
Value.
Claims (6)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110699701A (en) * | 2019-09-06 | 2020-01-17 | 华东理工大学 | A kind of nickel foam loaded with metal nickel and vanadium trioxide composite and its preparation method and application |
| CN111389429A (en) * | 2020-04-13 | 2020-07-10 | 苏州大学 | Preparation method of catalyst for catalyzing ammonia borane hydrolysis |
| CN111841589A (en) * | 2020-07-29 | 2020-10-30 | 浙江理工大学 | Nickel-cobalt-tungsten phosphide catalyst and preparation method and application thereof |
| CN113718278A (en) * | 2020-05-26 | 2021-11-30 | 湖南师范大学 | Preparation method of transition metal phosphorus/nitride heterojunction-based catalyst and efficient electrolytic water-evolution hydrogen research |
| CN114182289A (en) * | 2021-12-14 | 2022-03-15 | 黑龙江大学 | A kind of preparation method of molybdenum-nickel-based nitride of organic electro-oxidative coupling hydrogen evolution |
| CN114289043A (en) * | 2020-09-22 | 2022-04-08 | 新疆大学 | Preparation method and application of self-supporting porous nano-plate cobalt-nickel phosphide catalyst |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699701A (en) * | 2019-09-06 | 2020-01-17 | 华东理工大学 | A kind of nickel foam loaded with metal nickel and vanadium trioxide composite and its preparation method and application |
| CN111389429A (en) * | 2020-04-13 | 2020-07-10 | 苏州大学 | Preparation method of catalyst for catalyzing ammonia borane hydrolysis |
| CN111389429B (en) * | 2020-04-13 | 2023-04-11 | 苏州大学 | Preparation method of catalyst for catalyzing ammonia borane hydrolysis |
| CN113718278A (en) * | 2020-05-26 | 2021-11-30 | 湖南师范大学 | Preparation method of transition metal phosphorus/nitride heterojunction-based catalyst and efficient electrolytic water-evolution hydrogen research |
| CN111841589A (en) * | 2020-07-29 | 2020-10-30 | 浙江理工大学 | Nickel-cobalt-tungsten phosphide catalyst and preparation method and application thereof |
| CN111841589B (en) * | 2020-07-29 | 2023-07-25 | 浙江理工大学 | A kind of nickel cobalt tungsten phosphide catalyst and its preparation method and application |
| CN114289043A (en) * | 2020-09-22 | 2022-04-08 | 新疆大学 | Preparation method and application of self-supporting porous nano-plate cobalt-nickel phosphide catalyst |
| CN114182289A (en) * | 2021-12-14 | 2022-03-15 | 黑龙江大学 | A kind of preparation method of molybdenum-nickel-based nitride of organic electro-oxidative coupling hydrogen evolution |
| CN114182289B (en) * | 2021-12-14 | 2023-12-08 | 黑龙江大学 | Preparation method of molybdenum-nickel-based nitride for hydrogen evolution through electro-oxidative coupling of organic matters |
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